CN107447256A - A kind of method for preparing alkali formula magnesium iodide whisker - Google Patents
A kind of method for preparing alkali formula magnesium iodide whisker Download PDFInfo
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- CN107447256A CN107447256A CN201710640325.XA CN201710640325A CN107447256A CN 107447256 A CN107447256 A CN 107447256A CN 201710640325 A CN201710640325 A CN 201710640325A CN 107447256 A CN107447256 A CN 107447256A
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- whisker
- mixed liquor
- bittern
- solution
- magnesium iodide
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The invention discloses a kind of method for preparing alkali formula magnesium iodide whisker, comprise the following steps：S1. bittern is taken, filters and discards insoluble matter；S2. 3mol/L NaI solution is mixed for 3 ︰ 1 by volume with the bittern solution after step S1 processing, obtains mixed liquor 1；S3. mixed liquor 1 being heated to 30 DEG C, the NaOH solution that 0.8mol/L is then added dropwise into mixed liquor 1 under stirring obtains mixed liquor 2, wherein, the volume ratio of mixed liquor 1 and 0.8mol/L NaOH solution is 2.5~3.5：1；S4. mixed liquor 2 is continued under the conditions of 35 DEG C to be aged 55h, precipitation, drying alkali formula magnesium iodide whisker is collected by filtration.
Description
Technical field
The present invention relates to technical field of preparation for inorganic material, in particular it relates to a kind of side for preparing alkali formula magnesium iodide whisker
Method.
Background technology
China is a Salt production big country, and very long coastline provides guarantee for China's Salt production.The sea in China
Salt yield ranks first in the world, and produces 23000000 tons of sea salt, the annual m of by-product bittern 20,000,000 per year3, wherein magnesium chloride, magnesium sulfate
Stock number is respectively up to 379.2 ten thousand tons and 175.2 ten thousand tons.Although various chemical elements are more extra large in the bittern of by-product in salt-making process
Water concentrates 40 times or so, is the splendid raw material for extracting chemical element in seawater, but limited by technical merit, the utilization of bittern
Less than 20%, substantial amounts of bittern resource is discharged into sea or circulated in salt pan rate, had not only caused the waste of resource but also have impact on coastal waters sea
The ecological balance in domain.It is the effective measures for solving China's land resources deficiency to realize that bittern thoroughly comprehensively utilizes, and is to realize sea
Salt produces the necessary guarantee of energy-saving and emission-reduction, and the extremely urgent urgent problem of sea salt chemical industry.
Magnesium resource is quite abundant in bittern, and the concentration of magnesium ion is 60g/l, about 50 in seawater times in bittern, is system
The pole excellent raw material of standby magnesium salt whisker.When tradition prepares magnesium salt whisker, researcher is to be placed on notice how first to remove
Bittern impurity is removed, then goes to prepare expected material again, or is cleaned when preparing, or first tentatively obtained crude product,
Removal of impurities etc. is gone again.It is either any, due to there is the removal of impurities of complexity, thus infringement can be all brought to environment.So this " will
Utilize destruction Of resources environment, or do not utilize the good environment of protection of resources " contradictory relation become for develop resource section
Learn bottleneck problem.
First public Wu Jian pines in 2015 etc. directly using Guangdong Xuwen saltern bittern are raw material, bitter without purification ＆ isolation
Alkali lye is directly added into the case of halogen as precipitating reagent, be prepared for high-quality basic magnesium chloride whisker, alkali magnesium sulfate crystal whisker and
Basic magnesium carbonate whisker, eliminate extremely numerous and diverse dedoping step.But up to the present, it yet there are no and prepared without removal of impurities
The report of alkali formula magnesium iodide whisker.
The content of the invention
The invention aims to overcome the above-mentioned deficiency of prior art, there is provided a kind of alkali formula magnesium iodide whisker of preparing
Method.
To achieve these goals, the present invention is achieved by the following technical programs：
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. bittern is taken, filters and discards insoluble matter；
S2. 3mol/L NaI solution is mixed for 3 ︰ 1 by volume with the bittern solution after step S1 processing, mixed
Close liquid 1；
S3. mixed liquor 1 is heated to 30 DEG C, 0.8mol/L NaOH solution is then added dropwise into mixed liquor 1 under stirring
Mixed liquor 2 is obtained, wherein, the volume ratio of mixed liquor 1 and 0.8mol/L NaOH solution is 2.5~3.5：1；
S4. mixed liquor 2 is continued under the conditions of 35 DEG C to be aged 55h, precipitation, drying alkali formula magnesium iodide whisker is collected by filtration.
The present invention has found by studying, the only species of alkali lye, concentration, proportioning, the dosage ratio of alkali lye and bittern and
The addition sequence of alkali lye can influence the quality and yield of whisker, and the addition speed of alkali lye does not have for the quality and yield of whisker
Significant difference influences.
Preferably, the bittern derives from Cha Er Han Salt Lake, Leizhou saltern or Xuwen saltern.
Preferably, the volume ratio of the mixed liquor 1 and 0.8mol/L NaOH solution is 3：1.
Compared with prior art, the present invention has the advantages that：
The dosage ratio of species, concentration, proportioning of the invention by accurately controlling alkali lye, alkali lye and bittern, the addition of alkali lye are suitable
Sequence etc., meet whisker requirement so as to obtain draw ratio, whisker purity meets the alkali formula magnesium iodide whisker of commercial Application requirement.This hair
It is bright to be especially suitable for preparing alkali formula magnesium iodide whisker using the bittern in Qinghai Chaerhan salt lakes source as raw material.
Brief description of the drawings
Fig. 1 is that the SEM of alkali formula magnesium iodide whisker schemes.
Fig. 2 is the XRD diffraction patterns of alkali formula magnesium iodide whisker.
Embodiment
The present invention is made with reference to Figure of description and specific embodiment and further being elaborated, the embodiment
It is served only for explaining the present invention, is not intended to limit the scope of the present invention.Test method used in following embodiments is such as without spy
Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained
And material.
Inventor gathers bittern from Cha Er Han Salt Lake, Xuwen saltern and Leizhou saltern respectively, and determines various sources
The group of bittern wants component, the results are shown in Table 1.
Table 1 is the bittern principal component analysis result in three kinds of sources
Embodiment 1
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. 150mL mixed liquors 1 are taken, are placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
The NaOH solution 50mL into 0.8mol/L is slowly added dropwise under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, produces alkali formula magnesium iodide whisker.
XRD, SEM of measure gained whisker, elementary analysis result, SEM tests are shown to be crystal whisker-shaped（See Fig. 1）, XRD surveys
Test result is shown to be alkali formula magnesium iodide（See Fig. 2）, elementary analysis（It is shown in Table 2）It is shown to be the chemical formula of alkali formula magnesium iodide whisker：Mg2
(OH)3I·4H2O.Whisker yield is 90%, and whisker draw ratio is more than 10, whisker Functionality, quality and appealing design, complies fully with the demand of commercial Application.
The alkali formula magnesium iodide whisker Elemental analysis data of table 2
Embodiment 2
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. 100mL mixed liquors 1 are taken, are placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
It is added dropwise to 0.8mol/L NaOH solution 33mL slowly under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, alkali formula magnesium iodide whisker is produced, whisker yield is 91%, and whisker draw ratio is 16:1.
Embodiment 3
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 50mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, then
It is added dropwise to 0.8mol/L NaOH solution 17mL slowly under stirring, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, alkali formula magnesium iodide whisker is produced, whisker yield is 90%, and whisker draw ratio is 15:1.
Embodiment 4
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. it is that 3 ︰ 1 carry out mixing to obtain mixed liquor 1 by volume with bittern solution by NaI solution；
S4. take 25mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, then
It is added dropwise to 0.8mol/L NaOH solution 8.5mL slowly under stirring, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, alkali formula magnesium iodide whisker is produced, whisker yield is 92%, and whisker draw ratio is 16:1.Contrast
Example 1
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 1 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 150mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
It is added dropwise to 0.8mol/L NaOH solution 50mL slowly under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, this comparative example cannot get alkali formula magnesium iodide whisker.
Comparative example 2
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.2mol/L NaOH solution and 1.5mol/L NaI solution are prepared；
S3. 1.5mol/L NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 150mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
It is added dropwise to 0.2 mol/L NaOH solution 50mL slowly under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, this comparative example cannot get alkali formula magnesium iodide whisker.
Comparative example 3
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 150mL mixed liquors to be placed in 250mL conical flask, and conical flask is built in 80 DEG C of water-baths to 80 DEG C, then
It is added dropwise to 0.8mol/L NaOH solution 50mL slowly under stirring, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 55h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, this comparative example cannot get alkali formula magnesium iodide whisker.
Comparative example 4
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaI solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 150mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
It is added dropwise to 0.8mol/L NaOH solution 50mL slowly under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 5h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, this comparative example cannot get alkali formula magnesium iodide whisker.
Comparative example 5
A kind of method for preparing alkali formula magnesium iodide whisker, comprises the following steps：
S1. 300mL bitterns are taken（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
S2. 0.8mol/L NaOH solution and 3mol/L NaI solution are prepared；
S3. NaOH solution is mixed for 3 ︰ 1 by volume with bittern solution, obtains mixed liquor 1；
S4. take 150mL mixed liquors 1 to be placed in 250mL conical flask, and conical flask is built in 30 DEG C of water-baths to 30 DEG C, so
It is added dropwise to 3mol/L NaI Solutions Solution 50mL slowly under stirring afterwards, obtains mixed liquor 2；
S5. mixed liquor 2 is placed in the water-bath that water temperature is 35 DEG C and continued after being aged 5h, precipitation is collected by filtration, is placed in baking oven
（T=80±3℃,t=24h）Drying, the yield that this comparative example prepares alkali formula magnesium iodide whisker will be as a result undesirable less than 20%.
Claims (3)
- A kind of 1. method for preparing alkali formula magnesium iodide whisker, it is characterised in that comprise the following steps：S1. bittern is taken, filters and discards insoluble matter；S2. 3mol/L NaI solution is mixed for 3 ︰ 1 by volume with the bittern solution after step S1 processing, mixed Close liquid 1；S3. mixed liquor 1 is heated to 30 DEG C, 0.8mol/L NaOH solution is then added dropwise into mixed liquor 1 under stirring Mixed liquor 2 is obtained, wherein, the volume ratio of mixed liquor 1 and 0.8mol/L NaOH solution is 2.5~3.5：1；S4. mixed liquor 2 is continued under the conditions of 35 DEG C to be aged 55h, precipitation, drying alkali formula magnesium iodide whisker is collected by filtration.
- 2. described method according to claim 1, it is characterised in that the bittern is from Cha Er Han Salt Lake, Leizhou Saltern or Xuwen saltern.
- 3. described method according to claim 1, it is characterised in that the NaOH of the mixed liquor 1 and 0.8mol/L is molten The volume ratio of liquid is 3：1.
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| CN201710640325.XA CN107447256A (en) | 2017-07-31 | 2017-07-31 | A kind of method for preparing alkali formula magnesium iodide whisker |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935001A (en) * | 2017-12-25 | 2018-04-20 | 岭南师范学院 | A kind of method that alkali formula magnesium iodide whisker is produced in bittern from dried-up lake |
| CN107935002A (en) * | 2017-12-25 | 2018-04-20 | 岭南师范学院 | A kind of method that Basic magnesium bromide whisker is produced in bittern from dried-up lake |
| CN108103574A (en) * | 2017-12-25 | 2018-06-01 | 岭南师范学院 | A kind of method that Basic magnesium bromide whisker is prepared using seawater or bittern in salt lake |
| CN108118393A (en) * | 2017-12-25 | 2018-06-05 | 岭南师范学院 | A kind of method that magnesia crystal whisker is produced in bittern from dried-up lake |
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| CN101353815A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Method for preparing basic magnesium chloride whisker from dolomite and bittern |
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
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2017
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| CN101353815A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Method for preparing basic magnesium chloride whisker from dolomite and bittern |
| CN101353815B (en) * | 2008-08-19 | 2011-05-18 | 浙江大学 | Method for preparing basic magnesium chloride whisker from dolomite and bittern |
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935001A (en) * | 2017-12-25 | 2018-04-20 | 岭南师范学院 | A kind of method that alkali formula magnesium iodide whisker is produced in bittern from dried-up lake |
| CN107935002A (en) * | 2017-12-25 | 2018-04-20 | 岭南师范学院 | A kind of method that Basic magnesium bromide whisker is produced in bittern from dried-up lake |
| CN108103574A (en) * | 2017-12-25 | 2018-06-01 | 岭南师范学院 | A kind of method that Basic magnesium bromide whisker is prepared using seawater or bittern in salt lake |
| CN108118393A (en) * | 2017-12-25 | 2018-06-05 | 岭南师范学院 | A kind of method that magnesia crystal whisker is produced in bittern from dried-up lake |
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